Grain preparations of high diastatic power



Patented Nov. 1, 1949 GRAIN PREPARATIONS OF HIGH DIASTATIO POWER Victor L. Erlich, New York, N.- Y., assignor to Red Arrow. Malting Company, Milwaukee, Wis., a

limited partnership composed of Herbert Kurth and Katherine Kllrtll, both of Milwaukee, Wil.

No Drawing. Application April 6, 1945, Serial No. 587,006

1: Claims. (01. 195-64) This invention relates to grain preparations of high diastatic power and is applicable to the group of cereals described as the Hordeeae families, which comprises wheat, barley and rye. These cereals possess in their raw, mature state a certain but variable amount of active amylase of the saccharifying or so-called beta type. This active amylase, however, represents only a portion, usually less than one half or even less than one third of their potential or total amylase activity or diastatic power. This inactive, water insoluble portion of the total grain amylase can be' liberated in a higher or lesser degree upon germination of these grains either in nature or by melting.

It is known that the activation of the latent grain amylase can be done when the grain is finely ground and emulsifiedin water to which amylase activators are added. Proteolytic enzymes on the one hand, chemical compounds, particularlysulfur compounds of the reducing type such as sulfides or sulfites, and others have been described as activators. Analytical procedures are used to determine the potential total diastatic activity, which are based upon such activation of the finely ground grains in water mashes.

The present invention is based upon extensive experimental work which lead to the discovery that activation of the grain amylase can be obtained in any desired degree in the whole grains without germination on the one hand, or without crushing or milling the grains on the other.

The principal object of the present invention is to provide a whole grain product of high active diastatlc activity.

Another object is to provide a novel method of treating whole grains to increase the active diastatic power thereof.

Another object is to provide a method of converting substantially all of the inactive diastase diastatic power in whole grains.

In treating grains, in accordance with the present invention, the whole grains without being crushed or milled are steeped in water with additions of diastase activators. After steeping, the

and before drying.

The steeping of the grains consists in soaking the mechanically cleaned whole grains in the steep water for from a few hours to a usual maximum of approximately two days at suitable temperatures between 10 and preferably below C. Unlike usual steeping practice, the steep water does not have to be changed during. the operation. The determination of time and temperature are interdependent and governed by the particular grain being treated and the intended use of the finished product.

Practically all the various chemicals acting as diastase activators and proteolytic enzymes or both can be used, preference being given to those that are substantially soluble or emulsifiable in steeping water. For instance, reducing and/or proteolyzing agents are employed with good success.

As examples, sulfur dioxide, hydrogen sulfide, the various compounds containing or developing these groups, organic and inorganic sulfur compounds and the like can be used. Addition of acids like sulfuric, hydrochloric, lactic, acetic acid and the like has a favorable effect in some cases,

especially in view of regulating the pl-I of the the operation. Proteolytic enzymes like pepsinases. proteases and so on may be used in form of commercial papain, pepsin, yeast-autolysates etc.; here, bufieringagents like phosphates, calcium sulfate or other salts have their specific importance.

The duration of time of the steeping, necessary to obtain the highest yields of diastase activation depends largely upon the grain being treated, the

- activator employed and the temperature presteep liquor is separated from the swollen grains vailing in the steep. Higher temperatures accelerate the water absorption of the swelling grain and, accordingly,v the reactions necessary to activation. Different steeping times are employed for different grains to obtain the same amount of absorption, largely because of the difierent form and size of the grain and the quality of the husk and skin. For example, medium sized barley 3 requires approximately twice the time for complete swelling that is required by wheat.

Too long a steeping may result in undesirable leaching out of soluble compounds and soluble or solubilised enzymes and even in partial destruction of diastase. The same is true when too high a temperature'is employed for too' long a period.

Various temperatures may be employed within the suitable range at different periods of the steeping duration Increase in the concentration of the activators employed within limits speeds the reactions. Increase of concentration of the activators beyond suchlimits results in no further increase in the speed of diastase activation and in some instances may be detrimental.

The limits referred to differ with diflerent grains, activators, pH values. temperatures and can readily be determined in each instance by a few comparative tests.

The working conditions influence also the form and the solubility of the grain starch and the grain protein. For example, where greater protein solubili'zatlon is desired more emphasis has to be placed on the presence of proteolytic activators andparticularly of such enzymes. Where good filtering qualities are required for the finished product the maintenance of the pH value during steeping on the acid side between 3 and 6 has been found to be useful.

Where activation is to be done by both steep ing and germination, it is important to be careful as to the activating chemicals to be used, their concentration and other working conditions so that growth factors of the grain are not harmed.

In most cases, it is sufilcient and preferable to eliminate the expensive germination procedure and thereby greatly reduce the time and equipment required for malting.

The steeped wet grains can be crushed and used directly in mash treatments wherein the starch and other carbohydrate materials-are converted to hexoses and the like, as in the case when using normal green malts.

Where products for storage and shipment are to be prepared the steeped grains are dried or kilned at a temperature of not higher than 50 C. similar to the practice of drying green malt. Slow drying at low temperature sometimes even further increases the content of saccharogenic units in the final product, as determined by the Lintner test or other appropriate assays. The dried grains will have a moisture content between about four and ten per cent and will have an active diastatic power, in Lintner units. approximating and .in some instances even higher than that present in a kilned malt of the same grain variety prepared by former steeping and germination practices. The resulting product can be employed for many of the purposes and under the same working conditions as are usual for normal germinated malt. It is obvious that these activated grains can also be used simultaneously or in mixture with normal malt.

The equipment required for the steeping process is readily available in most grain processing plants, malteries. breweries, grain distilleries and the like. Stirring of the steeping grains may be provided for but if done it should be preferably without using aeration. The steeping liquid may be circulated over and through the grains. The usual kilns employed in malt houses for the drying of-malts can be used in drying the product of the present invention. Infrared radiation may be employed for drying the product.

Representative test runs on sample grains gave the results tabulated below. In carrying out these tests on the several grain varieties referred to the extract and protein content of the raw grain on a dry basis was first determined. The active diastatic power was determined according to the conventional Lintner test, and the total diastatic riods varying from 6 to 72 hours without changing the liquid. the quantity of which had been predetermined so as to furnish the desired complete water absorption by the grain with the swollen grain still under water. The temperature of the steep was maintained at a certain temperature level within the range of from 11 to 30 C. At the end of the chosen steeping times specified the liquid was drained and the grains washed thoroughly and rapidly with pure tap water. The wet grains were then dried in an' open air kiln within a temperature range of 35 to 45 C. down to a moisture content of l to 10% and average samples of the dried grains taken for analysis. Comparative tests were performed also on samples taken from the washed wet grains before drying. The results in Lintner degrees were in good accordance, with the wet grains giving in some cases figures of slightly lower values than that for the dried grains. The results'tabulated below are for tests on the dried material.

Example 1 Batches of a North Dakota hard spring wheat containing 75.7% extract and 17.5% total protein on a dry basis were treated as described within a temperature range of 1'! to 19 C. and gave the following results:

. Q The first figure in the column headed DH Imample 3 represents the pH at the hem Batches of one no variety containing 14.1%

and the second figure in each instance represents and 133% total protein on a dry has, the P at e end the steep- Th9 menu and of one barley variety containing 65.8% exbetween the fi ures in each ins n represents 5 tract and 18.1% total protein, were treated unthe efiective change in pH during the treatder similar conditions at 17 0.; the resulting ment. 1 dried grains gave the following results:

biestetic Power Duration 7 Actintoruaed 0mm 11 houra p T otel I" L Per cent of total Rye, Raw Grain me 125 51 I fill all 41 6.8to4.2 112 10.5 o) N808 0.1

a: as 8.0to7.2 21.5 82 89.6 3 12 1.010 100 95.5 05.5

Diastatio Power Aetiv ltoruled E pH 4 "quid hours I T ots] I" o L Per cent of total Bel-:5. Bur Groin. 142 66 46. 6 (a; nil 5e 1.0mm 124 01 40. (0 1:59.01 2.0 41 4.0 4.6 no 00 5.5

Example 2 trample 4 Batches of another hard wheat variety grown The following experimental data are given to in Minnesota and containing 81.1% extract and demonstrate the influence of both temperature 18.1% total protein on a dry basis, were treated during the steeping operation and its duration.

Diastatic Power Duration Per cent Active Activator used of Stee H V of liquid I L Per cent 01 Total 1 211 oz. 5 so 1111 4s 1 1. 2 to 4. 1 221 on v o. a 41 8.4 m 4. a 22s 40 {:8 41 4. s m a. 1 215 52 g; g 41 an to e. o 215 176 81.5 52 41 6.8 to 6.8 m 90.5

2. o 0.25 53 5.550111 188 184 as 1: 0 g 53 5.11050 11s an under similar conditions within a temperature The following figures refer to'batches of the range 01 17 to 19 C. same wheat variety as recorded in Example 2.

Diastatle Power I I Per cent Tempera- Dnmflm Active o L L. Per cent of total s. o n 24 2. 5 to a. 4. 200 128 64 Acetic Acld..-- o. 15 1s 24 a. a m 4. 1 192 112 so. 5

Pa 0.: u 48 a. a to 1. s 101 101 87. 5

1.5 a 22 8.4 to 1.0 189 158 ass as 48 8.4to 4.8 180 110 04.5

'7 The whole grain treated in accordance with the present invention has close to 1.00% of its diastatic potency in active form. The yield obtained by the process of the invention is substantially greater than that obtainable heretofore by any process of malting grains; the respiration loss and the loss due to rootlets and the like and which amount to from to of the weight of the original grain (on a dry time and the production cost are greatly reduced when compared with those required for the production of normal germinated malt. The prod-.

uct has practically the same over all composition as the raw grain since the chemicals used for the activation are removed. It can be employed in most cases like usual malt of comparable diastatic power.

1 have described what I believe .to be the preferred practice of my invention. I do not wish,

however, to be confined to the specific practice shown but what I desire to cover by Ietters Patent is set forth in the appended claims.

I claim: I

l. The process of transforming inactive diastase into active diastase in whole cereal grains of the Hordeeae families, comprising wheat, barley and rye prior to any breaking of the grains and prior to germination, comprising steeping the whole grain seeds in steep water containing amylase activators until the grains have reached an active diastatic power of at least 89% of their ing the whole grain seeds in the presence of water soluble chemical compounds which constitute amylase activators until the grains have reached an active diastatic power of at least 80% of their potential total diastatic power.

3. The process of transforming inactive diastase into active diastase in whole cereal grains of the Hordeeae families. comprising wheat, barley and rye prior to any breaking of the grains and prior to germination, comprising water steeping the whole grain seeds in the presence of proteolytic enzymes which act asamylase activators until the grains have reached an active diastatic power of at least 80% of their potential total diastatic power.

4. The process of transforming inactive diastase into active diastase in whole cereal grains of the Hordeeae families, comprising wheat, barley and rye prior to any breaking of the grains and prior to germination, comprising water steeping the whole grain seeds in the presence of proteolutic enzymes and of water soluble chemical compounds constituting amylase activators to activate both the proteolytic and amylolytic potentialities of the grains until the grains have reached an active diastatic power of at least 80% of their potential total diastatic power.

5. The process of transforming inactive diastase into active diastase in whole cereal grains of the Hordeeae families, comprising wheat, barley and rye prior to any breaking of .the grains and prior to germination, comprising water steeping the whole grain seeds in the presence of a sulflte compound in an amount corresponding to 80: concentrations of from about one-half to about three grams per one hundred milliliters of basis). is substantially-eliminated. The over all 10 8 steep liquor under conditions of temperature selected from the range oiiabout 10 C. to below 85 C.andofpHhigherthan8untilthedisstatic activityofthegrainsisatleast80% oftheir potential total diastatlc power.

6. The process of transforming inactive diastase into active diastase in whole cereal grains of the Hordeeae Yamilies, comprising wheat. barley and rye prior, to any breaking or the grains and prior to germination. comprising water steep-- ing the whole grain seeds in the presence of proteolytic enzymes of the papain type in concentrations corresponding to at least .2 gram of p psin per l00 milliliters of steep liquor and of added buffering agents to maintain the pH within a range of from 2 to about 8.5. until the diastaticactivity of the gralnsis at least 80% of their potential total diastatic power.

7. The process of transforming inactive diastase into active diastase in whole cereal grains of the Hordeeae families, comprising wheat. barley and rye prior to any breaking of the grains and prior tegermination. comprising water steeping the whole grain seeds in the presence of amylase activators until the grains have reached an active diastatic power of at least 80% of their potential total .diastatic power, and thereafter separating the whole grains from the steep liquor to terminate the steeping treatment and provide whole wet grains of increased diastatic activity as determined in degrees Lintner. R

8. A substantially non-germinated whole grain product of cereals belonging 'to the Hordeeae families comprising wheat, barley and rye, which in their raw state have a substantial amount of inactive amylase, comprising whole 'grains in which at least 80%. of their potential total diastatic power are activated as measured by the usual Lintner test.

9. A substantially non-germinated whole wheat grain product, comprising whole wheat grains of an active amylase content which is in excess of 80% of their potential total diastatic power as measured by the usual Iiintner test.

10. A-substantially non-germinated whole barley grain product, comprising whole barley grains of an active. amylase content which is in excess of 80% oftheir potential total diastatic power as measured by the usual Lintner test.

11. A substantially non-germinated whole rye grain product. comprising whole rye grains of an active amylase content which is in excess of 80% of their, potential total diastatic power as measured by the-usual Lintner test.

12. The process of transforming inactive diastase into active diastase in whole cereal grains of the Hordeeae families, comprising wheat, barley and rye prior to any breaking of the grains and prior to germination, comprising water steeping the whole grain seeds in the presence of amylase activators until the diastatic activity of the grains is at least 80% of their potential total diastatic power, separating the whole grains from the steep liquor to terminate the steeping treatment, and thereafter drying the grains at atem- VICTOR L'ERLICH.

(References on following Na 2,4ae,aae 9 REFERENCES CITED tlons, Cereal Chemistry 18 (1941). pages 113.20.

- Chemical Abstracts 30: 4881 (2) Chrzaszcz. The following references are of record in the and Janickl, Increase in the amount of active file of this patent: amylase in ungermlnated cereals by means of a H. s." m sums Imus Chemical Abstracts so: 1070 (2) Chrzaszcz and Number N m Date Janickl, "Protease action on protein of ungerml- 1,955,112 Curry Apr. 1 nated cereal grain and its eflect on the amylo- 2,228,717 Bergquist Jan. 14, 1941 lyflc power) 2,368,668 Iangtord et al. Feb. 6, 1945 10 Sumner et al.: Enzymes, Academic Press Inc.,

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